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Trifluoroacetic acid → HCID 22708205, Verbindung

HRID 1266532
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1266532
[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:40]=[CH:39][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([O:32]C(C)(C)C)=[O:31])=[CH:26][CH:25]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8].FC(F)(F)C(O)=O>ClCCl>[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:23][C:24]1[CH:25]=[CH:26][C:27]([O:28][C:29]([CH3:38])([CH3:37])[C:30]([OH:32])=[O:31])=[CH:39][CH:40]=1)[CH2:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:18])[CH3:17])=[CH:12][C:11]=1[C:19]([F:22])([F:21])[F:20])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 22708262HCID 22708262, Verbindung

Produkt 1

HCID 22708205HCID 22708205, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

0.842 g (1.49 mmol) of the compound from Example 3-7 is initially charged in 10 ml of dichloromethane. At room temperature, 10 ml of trifluoroacetic acid are added. The reaction mixture is stirred at room temperature for 2 hours. The mixture is then concentrated under reduced pressure using a rotary evaporator. The residue is taken up in ethyl acetate and washed with water, 20% strength sodium acetate solution, water and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent under reduced pressure. The product is purified chromatographically on silica gel (dichloromethane/methanol 30:1) and then dried under reduced pressure. This gives 0.648 g (85% of theory) of the title compound.

Aufarbeitung

  1. concentrationThe mixture is then concentrated under reduced pressure
  2. customa rotary evaporator
  3. washwashed with water, 20% strength sodium acetate solution, water and saturated sodium chloride solution
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. customThe product is purified chromatographically on silica gel (dichloromethane/methanol 30:1)
  6. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-988380cd7ee8422da7d0eaa609dbb0f8
Quelldatensatz
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06548538B2

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